Magnetic property studies and the crystallite structures evolution of spinel ferrite CoFe2O4 particles are reported in this paper. The ferrite was prepared through mechanical milling of all alloy precursors and sintered at various temperatures of 800, 900, 1000, and 1100 °C to promote the crystalline structure. X-ray diffraction (XRD) and Williamson-Hall plot were used to calculate the mean crystallite size and microstrain. Changes in the microstructure and crystallite sizes were occurring due to sintering treatments. It is found that the remanence (Mr) and saturation magnetization (Ms) increase with increasing sintering temperature, but a decrease occurred only at the temperature of 1100 °C. The optimum magnetic properties were obtained in a sample sintered at 1000 °C with a value of Mr = 36.00 emu/g and Ms = 74.05 emu/g.